TWI593631B - Apparatus for preparing germane gas and method for preparing monogermane gas using the same - Google Patents

Description

Zeoxane gas preparation device and method for preparing monodecane gas using same

The present invention relates to a decane gas producing apparatus and a method of producing a monodecane gas using the same. More particularly, the present invention relates to a decane gas producing apparatus capable of stably producing a large amount of monooxane gas by mixing a starting material in a short time, and using a reactor having a microstructured passage to simultaneously remove the heat of reaction, And a method of using the same to prepare a monodecane gas.

Germane gas is used in the semiconductor industry, which enables strained silicon to be used in computer central processing units and has become a key material for emerging germanium channels and gates. In addition, decane gas is used to form an intermediate SiGe layer of a triple junction of a fifth-generation amorphous germanium thin film solar cell (a-Si solar cell), thereby enhancing light for a medium wavelength range of 300-900 nm. Absorb and improve the efficiency of the battery. Accordingly, as the demand for next-generation thin-film solar cells is expected to increase, the demand for decane gas is expected to grow rapidly.

Since the 1930s, many chemists have studied the synthesis of decane gas and the chemical reactions involved. Typical examples include a chemical method of reducing cerium oxide (GeO 2 ) using a compound such as sodium borohydride (NaBH 4 ) or lithium aluminum hydride (LiAlH 4 ) or Neodymium tetrachloride (GeCl 4 ), an electrochemical method for the oxidation of cerium oxide, and a high energy method directly react cerium (Ge) with hydrogen.

As for the preparation of decane gas using ceria or ruthenium tetrachloride in the current method, the yield is only about 70%. In particular, when a monodecane gas is produced using cerium oxide which is easier to handle than ruthenium tetrachloride, it is difficult to prepare a monodecane gas at a high yield.

In view of the above, U.S. Patent No. 4,668,502 discloses the use of the same cerium oxide as a raw material by adjusting the reaction conditions, i.e., the concentration of cerium oxide, and the ratio of alkali/cerium oxide in an aqueous alkaline solution in which cerium oxide is dissolved. The combination of the amount of alkali metal borohydride, the concentration of the acid, the reaction temperature, and the like, the yield of the decane gas can be increased up to 97%. Indeed, when tested in accordance with the reaction conditions specified in the examples of U.S. Patent No. 4,668,502 and the scope of the patent application, about 90% of the high decane yield can be achieved.

However, according to the above method, the alkaline aqueous solution of the dissolved ceria and the alkali metal borohydride is reacted with the acidic aqueous solution in batch or continuously, and the decane gas is explosively generated in a short time, accompanied by High reaction heat. This means that if the preparation of decane gas is carried out on an industrial scale rather than on a laboratory scale, the reaction rate and heat of reaction will be difficult to control. If the high heat of reaction is not properly controlled, the reaction temperature will rise rapidly (about 50 ° C or higher), and higher decane may be formed, thus having a negative effect on the yield of monodecane.

The inventors of the present invention have made continuous efforts to solve the above problems. As a result, it was found that the problem can be solved by mixing the starting materials in a short time and using a reactor having one of the microstructure channels while removing the heat of reaction.

Method of synthesis of gaseous decane Germane, US 4,668,502)

Production method of germane (Production method of germane, JPA 1998-291804)

The present invention relates to a decane gas producing apparatus, and a method for producing a monodecane gas therewith, and more particularly to a decane gas producing apparatus by mixing a starting material in a short time and using a microstructured passage A reactor efficiently removes the heat of reaction while controlling the rapidly increasing temperature and pressure at which the decane gas is generated, has the ability to stably produce a large amount of monodecane gas, and a method of preparing a monodecane gas therefrom.

In a general aspect, the present invention provides a method for preparing a monodecane gas, comprising: implanting a cerium oxide (GeO 2 ) and an alkali metal hydride in a first channel and a second channel, respectively; a starting material alkaline aqueous solution and an acidic aqueous solution; mixing the injected starting material alkaline aqueous solution and the acidic aqueous solution in a third channel connecting one end of the first channel and one end of the second channel, and Reacting to produce a monodecane gas and a reaction solution; and discharging the produced monodecane gas and the reaction solution to the outside of the third channel, wherein the reaction heat generated in the third channel is caused by One of the coolants circulating in the coolant circulation unit adjacent to the third channel configuration is absorbed.

In an exemplary embodiment, the third channel can be a microchannel.

In an exemplary embodiment, the third passage may include a main passage and a plurality of parallel protruding projections formed on one side of the main passage. Preferably, the plurality of protruding portions may have an acute angle to the main passage and may protrude in one direction.

In an exemplary embodiment, the third channel can be maintained at a temperature of 0-50 °C.

In an exemplary embodiment, the temperature of the third passage can be controlled by adjusting at least one flow selected from the group consisting of a coolant, a temperature of the coolant, and a flow rate of the starting aqueous alkaline solution or the acidic aqueous solution.

In an exemplary embodiment, the heat of reaction generated in the third channel may be conducted to a first metal block surrounding one of the third channels, and the heat of reaction conducted to the first metal block may be conducted to The first metal block contacts one of the second metal blocks, and the heat of reaction conducted to the second metal block can be conducted to a coolant circulation unit surrounded by the second metal block, and the reaction to the coolant circulation unit Heat can be absorbed by one of the coolants circulating in the coolant circulation unit.

In an exemplary embodiment, the number of the third channels may be at least one, the at least one third channel may be connected in parallel, and the starting material alkaline aqueous solution and the acidic aqueous solution may be separately injected. The at least one of the third channels is configured to produce a monodecane gas in the at least one third channel.

In an exemplary embodiment, the alkali metal hydride can be sodium borohydride (NaBH 4 ).

In an exemplary embodiment, wherein the acidic aqueous solution may comprise an inorganic acid or an organic acid, wherein the inorganic acid may be one or more selected from the group consisting of sulfuric acid and phosphoric acid. The group, and the organic acid may be one or more selected from the group consisting of acetic acid and propionic acid.

In another general aspect, the present invention provides a decane gas preparation apparatus comprising: a first channel for injecting an alkaline aqueous solution of a starting material; a second channel for injecting an acidic aqueous solution; and connecting the first channel with a third channel of one end of the second channel, wherein the alkaline aqueous solution of the starting material and the acidic aqueous solution are mixed and reacted to generate a monodecane gas and a reaction solution; for the single channel generated in the third channel a decane gas and a discharge outlet through which the reaction solution is discharged; and a coolant circulation unit disposed adjacent to the third passage, and a coolant injected into and discharged from the coolant circulation unit, wherein the first The heat of reaction generated by the three channels is absorbed by the coolant.

In an exemplary embodiment, the third channel can be a microchannel.

In an exemplary embodiment, the third passage and the coolant circulation unit may be disposed apart from each other, the third passage may be surrounded by a first metal block, and the coolant circulation unit may be a second metal block Enclosing, and a configuration in which the first metal block and the second metal block are contactable with each other.

According to the present invention, the rapidly increasing temperature and pressure of the decane gas can be obtained by mixing the starting materials in a short period of time and using a reactor having a microstructured passage to efficiently remove the heat of reaction and control. And, according to the present invention, monodecane gas can be produced in a large amount and in high yield.

1‧‧‧ batch reactor

2‧‧‧Circulator

3‧‧‧ starting material alkaline aqueous reservoir

4‧‧‧Acid aqueous reservoir

5‧‧‧ coolant circulation unit

6‧‧‧Measuring pump

7‧‧‧ Recorder

8‧‧‧Emissions exports

10‧‧‧First Passage

20‧‧‧second channel

30‧‧‧ third channel

30a‧‧‧ main channel

30b‧‧‧ highlight

40‧‧‧Exhaust export

50‧‧‧ coolant circulation unit

55a‧‧‧ coolant inlet

55b‧‧‧ coolant discharge

60‧‧‧metal blocks

60a‧‧‧First metal block

60b‧‧‧Second metal block

Figure 1 is a representation of a batch reactor according to the prior art. intention.

Fig. 2a is an exploded view of one of the decane gas producing devices according to an exemplary embodiment of the present invention.

Fig. 2b is an assembled view of a decane gas producing apparatus according to an exemplary embodiment of the present invention.

Fig. 3a is a schematic view showing one of the third passages in the decane gas producing apparatus according to an exemplary embodiment of the present invention.

Fig. 3b is an enlarged view of one of the third passages in the decane gas producing apparatus according to an exemplary embodiment of the present invention.

Fig. 4 shows the temperature change of the third channel in the examples 1-4.

Fig. 5 shows changes in temperature of the third channel in Example 4 and Comparative Example 1.

Here, the present invention will be described in detail.

The term "micro-channel" as used in the present invention refers to a microstructured channel. The channel can have a diameter ranging from a few microns to a few thousand microns.

The term "reaction solution" as used in the present invention refers to a solution remaining after the alkaline aqueous solution of the starting material is reacted with an acidic aqueous solution to produce a decane gas.

A decane gas producing apparatus according to the present invention, comprising: a first channel 10 for injecting an alkaline aqueous solution of a starting material; a second channel 20 for injecting an acidic aqueous solution; and connecting to the first channel 10 and the second a third channel 30 at one end of the channel 20, and mixing and reacting the starting material alkaline aqueous solution and the acidic aqueous solution therein, To generate a monodecane gas and a reaction solution; a discharge outlet 40, the monodecane gas generated in the third passage and the reaction solution are discharged through the discharge outlet; and a coolant circulation unit 50 adjacent to the first A three-channel 30 configuration, and a coolant are injected into and discharged from the coolant circulation unit 50, wherein the heat of reaction generated by the third passage 30 is absorbed by the coolant. Specifically, the third channel 30 can be a microstructure channel. Specifically, the third passage 30 and the coolant circulation unit 50 may be spaced apart from each other, the third passage 30 may be surrounded by a first metal block 60a, and the coolant circulation unit 50 may be a second metal The block 60b surrounds, and the first metal block 60a and the second metal block 60b are arranged to be in contact with each other.

The first channel 10 is not limited to a specific aspect as long as the starting material alkaline aqueous solution is injected therein, and the injected starting material alkaline aqueous solution is transported to the third channel 30. Specifically, the first passage 10 may have a shape of a circular tube. Specifically, the first passage 10 can have corrosion resistance and acid resistance. The first passage 10 can be made of one or more materials selected from the group consisting of ceramics, stainless steel, titanium metal, and the like.

The starting material alkaline aqueous solution can be prepared by mixing cerium oxide (GeO 2 ) with an alkali metal hydride and an alkaline aqueous solution. The alkali metal hydride can be sodium borohydride (NaBH 4 ). The method of preparing the alkaline aqueous solution of the starting material is not limited to a specific aspect. For example, the starting material alkaline aqueous solution, as described in U.S. Patent No. 4,668,502, may be prepared by adding an alkali metal hydride powder to a metal hydroxide aqueous solution of cerium oxide (GeO 2 ), or It is prepared by previously preparing a predetermined concentration of an aqueous alkaline solution and subsequently adding cerium oxide powder and an alkali metal hydride thereto. In the alkaline aqueous solution of the starting material used in the present invention, the concentration of cerium oxide may specifically be not more than 0.5 mol/L, more specifically 0.3 mol/L. Specifically, every 1 mol of cerium oxide, It may contain 2 or more equivalents of the metal hydroxide, and may contain 4 mol or more of the alkali metal hydride per 1 mol of cerium oxide. Outside of the above range, it is possible to reduce the conversion ratio of cerium oxide and thus the economic efficiency of monodecane gas production. The alkaline aqueous solution may be an aqueous alkali metal solution or an alkaline earth metal aqueous solution, specifically an aqueous NaOH solution or an aqueous KOH solution. If an aqueous solution of NaOH is used and if a basic aqueous solution of the starting material is prepared using NaBH 4 as an alkali metal hydride, hydrogen is not produced because NaBH 4 is stabilized.

The second passage 20 is not limited to a specific aspect as long as the acidic aqueous solution is injected therein, and the injected acidic aqueous solution is transported to the third passage 30. Specifically, the first passage 10 may have a shape of a circular tube. Specifically, the second passage 20 may have corrosion resistance and acid resistance. The second passage 20 may be made of one or more materials selected from the group consisting of ceramics, stainless steel, titanium metal, and the like.

The acidic aqueous solution can be prepared by mixing an acid selected from a mineral acid (e.g., sulfuric acid and phosphoric acid) or an organic acid (e.g., acetic acid, propionic acid, etc.) with water. Specifically, the use of a volatile acid such as hydrochloric acid can be avoided in consideration of purification of a monodecane gas. The acidic aqueous solution is not limited to a specific concentration.

The third channel 30 is not limited to a specific aspect as long as it is connected to one end of the first channel 10 and one end of the second channel 20, and the alkaline aqueous solution is mixed and reacted with the acidic aqueous solution. Specifically, the third channel 30 can be a microstructure channel. The diameter and length of the microstructure channel can vary depending on the size of the device and the throughput required for the decane gas. Specifically, it may be between several tens of microns and several hundred microns.

The third channel 30 can include a main channel 30a and is configured A plurality of protruding portions 30b projecting in parallel on one side of the main passage. The plurality of protruding portions 30b may have an acute angle to the main passage and may protrude in one direction. By including the main passage 30a and the protruding portion 30b, the third passage 30 can continuously move the fluid passing therethrough upward and downward, and the fluid can be split or recombined. With such a configuration, the third channel 30 can not only easily mix the aqueous starting material solution injected from the first channel 10 and the second channel 20 with the acidic aqueous solution, but also the aqueous solution of the starting material and the acid. The increase in the contact area of the aqueous solution also promotes the production of decane gas. The third channel 30 can further include a temperature sensor (not shown). The temperature sensor can perform an immediate temperature measurement of the third passage 30, whereby the reaction temperature and the flow rate of the coolant through the coolant circulation unit 50 can be easily controlled, thereby increasing the yield of the monodecane gas.

The discharge outlet 40 is not limited to a specific aspect as long as the decane gas and the reaction solution generated in the third passage 30 can be discharged out of the third passage 30. The discharge outlet 40 is coupled to one end of the third passage 30 and, in particular, may have the shape of a circular tube. The diameter of the discharge outlet 40 connected to one end of the third passage 30 can be varied depending on the size of the apparatus and the amount of production required for the decane gas.

The coolant circulation unit 50 can be disposed adjacent to the third passage 30. It contains a coolant inlet 55a for coolant injection and a coolant discharge outlet 55b for coolant discharge. It is not limited to a specific aspect as long as the coolant that absorbs the heat of reaction generated in the third passage 30 can pass therethrough. The coolant circulation unit 50 can be a linear or zig-shaped conduit through which the coolant can pass. The diameter of the coolant circulation unit 50 can be varied depending on the size of the apparatus and the amount of production required for the decane gas.

The coolant circulating in the coolant circulation unit 50 is not limited to a special one. The stationary state is as long as it is permeable to the coolant discharge inlet 55a located at one end of the coolant circulation unit 50 and is discharged through the coolant discharge outlet 55b located at the other end of the coolant circulation unit 50, and It solidifies at a temperature of 0 ° C or lower. Specifically, it may be ethylene glycol.

In an exemplary embodiment, the third passage 30 and the coolant circulation unit 50 may be disposed apart from each other, the third passage may be surrounded by a first metal block 60a, and the coolant circulation unit 50 may be The second metal block 60b surrounds, and the first metal block 60a and the second metal block 60b are disposed in contact with each other. In the exemplary embodiment, the heat of reaction generated in the third channel 30 is conducted to the first metal block 60a surrounding the third channel, and the heat of reaction conducted to the first metal block 60a is conducted to the The second metal block 60b that the first metal block 60a contacts, and the heat of reaction conducted to the second metal block 60b are conducted to the coolant circulation unit 50 surrounded by the second metal block 60b. The heat of reaction conducted to the coolant circulation unit 50 is absorbed by the coolant circulated in the coolant circulation unit 50.

The first metal block 60a is not limited to a specific aspect as long as it surrounds the third channel 30. Specifically, it can be made of a metal material having high thermal conductivity. The second metal block 60b is not limited to a specific aspect as long as it surrounds the coolant circulation unit 50. Specifically, it can be made of a metal material having high thermal conductivity.

In an exemplary embodiment, the first metal block 60a and the second metal block 60b may have a rectangular shape. If the first metal block 60a and the second metal block 60b have a larger contact area, heat of reaction may preferably be conducted from the third channel 30 to the coolant circulation unit 50.

Step 1: Injecting of the basic raw material aqueous solution and the acidic aqueous solution First, an alkaline aqueous solution containing a starting material of cerium oxide (GeO 2 ) and an alkali metal hydride, and an acidic aqueous solution are injected into a first passage 10 and a second passage 20, respectively.

The alkaline aqueous solution of the starting material injected into the first passage 10 can be prepared by mixing cerium oxide (GeO 2 ) with an alkali metal hydride and an alkaline aqueous solution. The alkali metal hydride can be NaBH 4 . The starting material alkaline aqueous solution, as described in U.S. Patent No. 4,668,502, may be prepared by adding an alkali metal hydride powder to a metal hydroxide aqueous solution of cerium oxide (GeO 2 ) or by pre-preparation. A predetermined concentration of an aqueous alkaline solution and subsequent addition of cerium oxide powder and an alkali metal hydride are prepared, but the present invention is not limited to the above. In the alkaline aqueous solution of the starting material used in the present invention, the concentration of cerium oxide may specifically be not more than 0.5 mol/L, more specifically 0.3 mol/L. Each 1 mol of cerium oxide may contain 2 or more equivalents of the metal hydroxide, and may contain 4 or more moles of the alkali metal hydride per 1 mol of cerium oxide. Outside of the above range, it is possible to reduce the conversion ratio of cerium oxide and thus the economic efficiency of monodecane gas production. The alkaline aqueous solution may be an aqueous alkali metal solution or an alkaline earth metal aqueous solution, specifically an aqueous NaOH solution or an aqueous KOH solution. If an aqueous solution of NaOH is used and if a basic aqueous solution of the starting material is prepared using NaBH 4 as an alkali metal hydride, hydrogen is not produced because NaBH 4 is stabilized.

The acidic aqueous solution injected into the second passage 20 can be prepared by mixing an acid selected from a mineral acid (e.g., sulfuric acid and phosphoric acid) or an organic acid (e.g., acetic acid and propionic acid) with water. Specifically, the use of a volatile acid such as hydrochloric acid can be avoided in consideration of purification of a monodecane gas. The acidic aqueous solution is not limited to a specific concentration.

The injection rate of the alkaline aqueous solution of the starting material and the acidic aqueous solution It can be tens of milliliters per minute. The injection rate can be varied depending on the size of the device and the throughput required for the decane gas.

The alkaline aqueous solution of the starting material and the acidic aqueous solution may be injected into the first passage 10 and the second passage 20 by using any means capable of continuously injecting the alkaline aqueous solution of the starting material and the acidic aqueous solution, and is not limited to a specific one. Aspect. Specifically, a metering pump or the like can be used.

Step two

The raw material alkaline aqueous solution and the acidic aqueous solution respectively injected into the first channel 10 and the second channel 20 are respectively transmitted through the channel to a third channel connecting one end of the first channel 10 and one end of the second channel 20 30. In the third passage 30, the transported starting material alkaline aqueous solution is mixed with the acidic aqueous solution, and the generation of decane gas occurs at the interface where they contact each other.

Specifically, the third channel 30 in which the reaction occurs may be a microchannel. In the case of a microchannel, the third channel 30 promotes the production of decane gas and maximizes the effect of controlling the temperature rise caused by the reaction heat generated. This is because the generation of decane gas occurs only at the interface where the starting aqueous alkaline solution and the acidic aqueous solution contact each other. That is, the area where the two solutions contact each other as the solution is reduced to the droplet size, so that the area of the area increases and the number increases, making it easier to mix on the micrometer scale.

The third passage 30 may include a main passage 30a and a plurality of parallel protruding projections 30b formed on one side of the main passage. The plurality of protruding portions 30b may have an acute angle to the main passage and may protrude in one direction. According to this, the alkaline aqueous solution and the acidic aqueous solution of the starting material respectively injected into the third channel 30 can be respectively in the main The passage 30a and the projection 30b are continuously moved upward and downward, and are separated or recombined. As a result, the starting aqueous alkaline solution is mixed with the acidic aqueous solution at a micrometer scale, and the interface is mutually reacted to produce a decane gas.

The heat of reaction is generated when decane gas is generated. Due to the heat of reaction, the temperature in the third passage 30 may rise rapidly. To solve this problem, a coolant circulation unit 50 is disposed adjacent to the third passage 30 to absorb the heat of reaction when the reaction occurs.

In an exemplary embodiment, decane gas is generated in the third passage 30, and the heat of reaction generated when the decane gas is generated is conducted to the first metal block 60a surrounding one of the third passages 30. The first metal block 60a conducts the heat of reaction to one of the second metal blocks 60b in contact with the first metal block 60a. The heat of reaction conducted to the second metal block 60b is conducted to the coolant circulation unit 50 surrounded by the second metal block 60b. The heat of reaction conducted to the coolant circulation unit 50 is absorbed by a coolant circulating in the coolant circulation unit 50. The absorption of the heat of the reaction can be controlled by regulating the temperature and flow rate of the coolant supplied to the coolant circulation unit. If the amount of the alkaline aqueous solution of the starting material and the acidic aqueous solution is increased in order to increase the generation of the decane gas, the third passage 30 may be maintained by lowering the temperature of the coolant or by increasing the flow rate of the coolant. The internal reaction temperature is constant.

The temperature in the third passage 30 can be controlled by adjusting the flow rate selected from at least the coolant, the temperature of the coolant, and the flow rate of the starting aqueous alkaline solution or the acidic aqueous solution. The temperature in the third passage can be specifically maintained at a temperature of 50 ° C or lower, more specifically 0-50 ° C. If the temperature is high, the reaction of the basic aqueous solution of the starting material with the acidic aqueous solution may promote the formation of higher decane rather than monodecane, and thus has a negative effect on the yield of the monodecane gas.

In an exemplary embodiment, the number of the third channels 30 may be at least one, the at least one third channel 30 may be connected in parallel, and the starting material alkaline aqueous solution and the acidic aqueous solution may be respectively separated. The at least one third channel 30 is implanted to generate monodecane gas in the at least one third channel 30. If the third passages 30 are connected in parallel, a large amount of monodecane gas can be produced on an industrial scale.

Step three

The monodecane gas and the reaction solution produced by the reaction are discharged through the discharge port 40 connected to one end of the third passage 30 to discharge the third passage 30. The discharged monodecane gas is separately collected in the reaction solution. Through the above steps, the production of monodecane gas can have a high yield of 90% or higher.

When a current batch reactor or a continuous reactor is used, even if the coolant circulates in the cooling jacket surrounding the reactor, it is difficult to control the temperature rise caused by the heat of reaction generated by the formation of decane gas inside the reactor.

However, the advantage of the reactor comprising a microstructured channel according to the present invention is not only that it is easier to mix and react the starting aqueous alkaline solution or the acidic aqueous solution, but also because the temperature of the reactor can be maximized due to the cooling effect. It is easily maintained at 0-50 °C. Therefore, a large amount of monodecane gas can be produced in a high yield.

Hereinafter, the present invention will be described in detail through examples. However, the following examples are for illustrative purposes only, and those skilled in the art can clearly understand the scope of the invention, and the scope of the invention is not limited to the embodiments.

An acidic aqueous solution was prepared by dissolving 75 g of concentrated sulfuric acid (96%, H 2 SO 4 ) in 500 mL of distilled water at 20 °C.

Dissolve 2.28 mL of 50% NaOH in 20 ° C In 250 mL of distilled water, 3.4 g of cerium oxide (GeO 2 ) and 7.4 g of NaBH 4 were sequentially dissolved in the above-obtained solution to prepare a starting aqueous alkaline solution.

The starting aqueous alkaline solution was injected into the first passage 10 in a decane gas producing apparatus (see Fig. 2a) according to an exemplary embodiment of the present invention at a rate of 8 mL/min. At the same time, the acidic aqueous solution was injected into a second passage 20 at a rate of 16 mL/min. The above solution was injected using a metering pump. A device is used to measure the rise in temperature as the decane gas is produced. The temperature of the reaction solution discharged through the discharge outlet 40 connected to one of the third passages 30 is measured.

When the temperature of the third passage 30 is maintained constant, the circulation of the refrigerant circulation unit of the decane gas producing apparatus with ethylene glycol as a coolant is started. The temperature in the third passage 30 is maintained at about 38 ° C at which temperature the cycle of ethylene glycol begins. The ethylene glycol was supplied at a flow rate of 15 ° C and 120 mL / min. When the circulation of the coolant is started, the temperature of the third passage 30 drops rapidly and is maintained at about 23 °C.

The flow rate of the alkaline aqueous solution of the starting material and the acidic aqueous solution was increased by 2, 3 and 4 times, and the other conditions were maintained as in Example 1.

In Example 2, the temperature of the third passage 30 was maintained at 42 °C. When ethylene glycol is supplied at 5 ° C, the temperature of the third passage 30 drops rapidly and is maintained at about 28 ° C (see Figure 4).

In Example 3, the temperature of the third passage 30 was maintained at 43 °C. When ethylene glycol is supplied at -5 ° C, the temperature of the third passage 30 drops rapidly and is maintained at about 30 ° C (see Figure 4).

In Example 4, the temperature of the third passage 30 was maintained at 43 °C. When ethylene glycol is supplied at -10 ° C, the temperature of the third passage 30 drops rapidly, maintaining at about 32 °C (see Figure 4).

A starting material alkaline aqueous solution and an acidic aqueous solution were prepared in the same manner as in Example 1.

The starting aqueous alkaline solution and the acidic aqueous solution were injected into a 1 liter glass reactor using a metering pump at the same flow rate as in Example 4.

When the temperature of the 1 liter glass reactor reached 43 ° C, ethylene glycol (coolant) was circulated at a flow rate of -10 ° C and 250 mL / min (see Figure 5).

Comparing the results of Comparative Example 4 with Comparative Example 1, when the decane gas producing apparatus of the present invention (Example 4) was used, the coolant ethylene glycol was remarkably improved as compared with the use of the current reactor (Comparative Example 1). Cooling effect. Thanks to this excellent cooling effect, it is easier to maintain the temperature suitable for the preparation of monodecane gas (ie, 0-50 ° C) by controlling the heat of reaction generated when mass producing decane gas (see Figure 5).

Accordingly, it can be seen that the decane gas producing apparatus and the monodecane gas producing method according to the present invention have an advantage not only in mixing and reacting the reactant but also in controlling the reaction temperature which rises due to the heat of reaction. Thereby, a large amount of monodecane gas can be produced in a high yield.

While the present invention has been shown and described, it will be understood that

10‧‧‧First Passage

20‧‧‧second channel

30‧‧‧ third channel

40‧‧‧Exhaust export

50‧‧‧ coolant circulation unit

55a‧‧‧ coolant inlet

55b‧‧‧ coolant discharge

60a‧‧‧First metal block

60b‧‧‧Second metal block

Claims (12)

A method for preparing a monodecane gas comprises: injecting an alkaline aqueous solution containing a starting material of cerium oxide (GeO2) and an alkali metal borohydride (MBH4) and an acid in a first channel and a second channel, respectively An aqueous solution; in a third channel connecting one end of the first channel and one end of the second channel, mixing the injected raw material alkaline aqueous solution and the acidic aqueous solution, and reacting it to generate a monodecane gas and a a reaction solution; and discharging the produced monodecane gas and the reaction solution to the outside of the third passage, wherein the heat of reaction generated in the third passage is due to a coolant disposed adjacent to the third passage A coolant is circulated in the circulation unit for absorption, and wherein the third passage is a microchannel. The method for producing a monodecane gas according to claim 1, wherein the third channel comprises a main channel and a plurality of parallel protruding protrusions formed on one side of the main channel. The method for producing a monodecane gas according to claim 2, wherein the plurality of protruding portions have an acute angle to the main passage and protrude in one direction. The method for producing a monodecane gas according to claim 1, wherein the temperature of the third channel is maintained at 0-50 °C. The method for preparing a monodecane gas according to claim 4, wherein the temperature of the third passage is controlled by at least one flow selected from the coolant, cold The temperature of the agent and the flow rate of the alkaline aqueous solution or the acidic aqueous solution of the starting material are controlled. The method for preparing a monodecane gas according to claim 1, wherein the heat of reaction generated in the third channel is conducted to a first metal block surrounding one of the third channels, and the conduction to the first metal The heat of reaction of the block is conducted to a second metal block in contact with the first metal block, the heat of reaction conducted to the second metal block being conducted to a coolant circulation unit surrounded by the second metal block, and the conduction to The heat of reaction of the coolant circulation unit is absorbed by the coolant circulating in the coolant circulation unit. The method for preparing a monodecane gas according to claim 1, wherein the third channel is at least one, the at least one third channel is connected in parallel, and the starting material alkaline aqueous solution and The acidic aqueous solution is separately injected into the at least one third passage to facilitate the production of monodecane gas in the at least one third passage. The method for producing a monodecane gas according to claim 1, wherein the alkali metal hydride is NaBH 4 . The method for producing a monodecane gas according to claim 1, wherein the acidic aqueous solution comprises an inorganic acid or an organic acid, wherein the inorganic acid is one or more selected from the group consisting of sulfuric acid and phosphoric acid. The group, and one or more of the organic acid systems, are selected from the group consisting of acetic acid and propionic acid. A decane gas preparation device comprising: a first channel for injecting an alkaline aqueous solution of a starting material; a second channel for injecting an acidic aqueous solution; and a first end connected to one end of the first channel and one end of the second channel a three-channel, wherein the alkaline aqueous solution of the starting material and the acidic aqueous solution are mixed and reacted to generate a monodecane gas and a reaction solution; the monodecane gas generated in the third channel is passed through the reaction solution a discharge outlet for discharging; and a coolant circulation unit disposed adjacent to the third passage, and a coolant injected into and discharged from the coolant circulation unit, wherein the reaction heat generated by the third passage is The coolant is absorbed, wherein the alkaline aqueous solution of the starting material comprises cerium oxide (GeO2) and alkali metal borohydride (MBH4), and wherein the third channel is a microchannel. The decane gas producing apparatus according to claim 10, wherein the third channel is a microchannel. The decane gas producing apparatus according to claim 10, wherein the third passage and the coolant circulation unit are disposed apart from each other, and the third passage is surrounded by a first metal block, the coolant circulation unit Surrounded by a second metal block, and the first metal block and the second metal block are in contact with each other.